An analytical method for multiclass determination of steroid hormones in compost has been developed to fill the lack of methods for steroid residuals monitoring in this waste-derived product, increasingly produced and recycled in the circular-economy approach. The procedure simply entails an ultrasound-assisted extraction (UAE) on 300 mg compost by 3 × 2.5 mL methanol × 5 min sonication steps followed by a quick clean-up by solid-phase extraction (SPE) on the silica-based Supelclean™ LC-NH2 that avoids use of organic solvents. The clean extract is analysed by HPLC-MS/MS achieving firm identification and quantitation of the 16 steroids, i.e., glucocorticoids, progestins, androgens, oestrogens. The analytical figures of merits were assessed, viz. selectivity, sensitivity, linearity, matrix effect, trueness, precision, carry-over and robustness, in line with updated guidelines. Recovery was investigated in the concentration range 15–800 ng g−1, and at the quality control levels (15, 50, 200 and 400 ng g−1) was in the range 60–120%, with inter-day precision RSDs < 20% (n = 3). The experimental quantification limit was 15 ng g−1 for all the hormones. The method was applied to analysis of different compost samples proving to be functional to environmental monitoring.

Multiclass ultrasound-assisted extraction, clean-up and high performance liquid chromatography-tandem mass spectrometry quantification of steroid hormone residues in compost

Speltini A.
;
Merlo F.;Maraschi F.;Bianchini P.;Mandri A.;Profumo A.
2023-01-01

Abstract

An analytical method for multiclass determination of steroid hormones in compost has been developed to fill the lack of methods for steroid residuals monitoring in this waste-derived product, increasingly produced and recycled in the circular-economy approach. The procedure simply entails an ultrasound-assisted extraction (UAE) on 300 mg compost by 3 × 2.5 mL methanol × 5 min sonication steps followed by a quick clean-up by solid-phase extraction (SPE) on the silica-based Supelclean™ LC-NH2 that avoids use of organic solvents. The clean extract is analysed by HPLC-MS/MS achieving firm identification and quantitation of the 16 steroids, i.e., glucocorticoids, progestins, androgens, oestrogens. The analytical figures of merits were assessed, viz. selectivity, sensitivity, linearity, matrix effect, trueness, precision, carry-over and robustness, in line with updated guidelines. Recovery was investigated in the concentration range 15–800 ng g−1, and at the quality control levels (15, 50, 200 and 400 ng g−1) was in the range 60–120%, with inter-day precision RSDs < 20% (n = 3). The experimental quantification limit was 15 ng g−1 for all the hormones. The method was applied to analysis of different compost samples proving to be functional to environmental monitoring.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11571/1475115
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